CN104559511A - Organic-inorganic compound water based paint and preparation method thereof - Google Patents
Organic-inorganic compound water based paint and preparation method thereof Download PDFInfo
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- CN104559511A CN104559511A CN201510014353.1A CN201510014353A CN104559511A CN 104559511 A CN104559511 A CN 104559511A CN 201510014353 A CN201510014353 A CN 201510014353A CN 104559511 A CN104559511 A CN 104559511A
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- 239000003973 paint Substances 0.000 title claims abstract description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910010272 inorganic material Inorganic materials 0.000 title abstract 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 54
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 51
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims abstract description 50
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000839 emulsion Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 27
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 26
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000001632 sodium acetate Substances 0.000 claims abstract description 24
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 24
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 69
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 46
- 239000002131 composite material Substances 0.000 claims description 39
- 239000006185 dispersion Substances 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 26
- 239000012621 metal-organic framework Substances 0.000 claims description 26
- 239000012875 nonionic emulsifier Substances 0.000 claims description 25
- 239000013530 defoamer Substances 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 23
- 235000012239 silicon dioxide Nutrition 0.000 claims description 23
- 235000019353 potassium silicate Nutrition 0.000 claims description 15
- 229920002401 polyacrylamide Polymers 0.000 claims description 10
- 229950002895 cellaburate Drugs 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 4
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract 1
- 229920001909 styrene-acrylic polymer Polymers 0.000 abstract 1
- 238000000576 coating method Methods 0.000 description 17
- 239000011248 coating agent Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 9
- 125000005375 organosiloxane group Chemical group 0.000 description 8
- 238000001035 drying Methods 0.000 description 6
- 230000001804 emulsifying effect Effects 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000009970 fire resistant effect Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- -1 polyoxyethylene nonylphenol Polymers 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000013132 MOF-5 Substances 0.000 description 1
- 229910002656 O–Si–O Inorganic materials 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003254 anti-foaming effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012703 microemulsion polymerization Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000005028 tinplate Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention provides organic-inorganic compound water based paint and a preparation method thereof. The organic-inorganic compound water based paint is prepared from the following raw materials: water, iron powder, benzene 1,3,5-tricarboxylic acid, hydrofluoric acid, nitric acid, N,N-dimethyl formamide, sodium silicate, non-ionic emulsion, styrene-acrylic emulsion, silica sol, nano-titanium dioxide dispersoid, sodium acetate, a defoaming agent, a flatting agent, a dispersing agent and talcum powder. Compared with the prior art, the organic-inorganic compound water based paint has the advantages that water soluble sodium silicate is taken as an inorganic film forming matter and then is compounded with a metal organic frame (MOF) material, thus obtaining the organic-inorganic compound water based paint; and the MOF material has the unique characteristics that thermal stability is good, an open-framework structure is ordered and functional group modification can be carried out in pores and on the surfaces, so that the water based paint has good stability, high temperature resistance and adhesion.
Description
Technical field
The present invention relates to technical field of coatings, particularly relate to a kind of Organic-inorganic composite water-miscible paint and preparation method thereof.
Background technology
Along with the development of industrial technology, high-temperature-resistant thermal-insulation thermal insulating coating arises at the historic moment, and water-miscible paint receives much concern because of its many premium properties, and it has considerable development trend in the use in high temperature resistant field.At present, water-miscible paint can be coated in the higher aspect of surface temperature, and as high temperature metal partss such as oven, electromagnetic oven, heat exchangers, but its sticking power and resistance to elevated temperatures need to improve further.
In general, high-temperature resistant coating is mainly divided into organic high temperature-resistant coating, refractory inorganic paint and Organic-inorganic composite high-temperature resistant coating.Complex fire resistant coating is mainly divided into two classes, and a class does film forming matter with organism (resin or emulsion), in system, then adds a large amount of mineral powders do color stuffing, be i.e. inorganic component.Another kind of is take inorganic component as substrate, the resistance to elevated temperatures of inorganic component is better, generally can bear the temperature of 400 ~ 1000 DEG C, but film forming curing performance is poor, water tolerance, sticking power, impact strength are poor, therefore, in inorganic component, add silicone resin solve the problem, obtain organic-inorganic hybrid coatings.
In prior art, application number be 01136262.6 Chinese patent literature report a kind of high-temp .-resisting fire-proof composite nano paint, comprise nanometer silicon carbide, nano silicate clay, phosphoric acid salt, nanometer aluminium silicate and organic polymer material.But the sticking power of this high-temp .-resisting fire-proof composite nano paint is poor, and this high-temperature behavior awaits further raising.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of Organic-inorganic composite water-miscible paint and preparation method thereof, and it has good resistance to elevated temperatures and stronger sticking power.
In view of this, the invention provides a kind of Organic-inorganic composite water-miscible paint, prepared by following raw material: water 25 ~ 45 weight part, iron powder 1 ~ 3 weight part, 1, 3, 5-benzenetricarboxylic acid 2 ~ 6 weight part, hydrofluoric acid 0.05 ~ 0.1 weight part, nitric acid 0.05 ~ 0.1 weight part, N, dinethylformamide 0.2 ~ 0.6 weight part, water glass 30 ~ 40 weight part, non-ionic emulsifier liquid 0.2 ~ 0.3 weight part, benzene emulsion 2 ~ 8 weight part, silicon dioxide gel 5 ~ 10 weight part, nano titanium oxide dispersion 3 ~ 8 weight part, sodium acetate 0.1 ~ 0.2 weight part, defoamer 0.15 ~ 0.3 weight part, flow agent 0.15 ~ 0.3 weight part, dispersion agent 1 ~ 1.5 weight part, talcum powder 10 ~ 13 weight part.
Preferably, prepared by following raw material: water 30 ~ 40 weight part, iron powder 2 ~ 3 weight part, 1, 3, 5-benzenetricarboxylic acid 4 ~ 5 weight part, hydrofluoric acid 0.05 ~ 0.1 weight part, nitric acid 0.05 ~ 0.1 weight part, N, dinethylformamide 0.3 ~ 0.5 weight part, water glass 30 ~ 35 weight part, non-ionic emulsifier liquid 0.25 ~ 0.3 weight part, benzene emulsion 3 ~ 5 weight part, silicon dioxide gel 6 ~ 8 weight part, nano titanium oxide dispersion 4 ~ 6 weight part, sodium acetate 0.15 ~ 0.2 weight part, defoamer 0.2 ~ 0.3 weight part, flow agent 0.15 ~ 0.2 weight part, dispersion agent 1 ~ 1.5 weight part, talcum powder 11 ~ 13 weight part.
Accordingly, the present invention also provides a kind of preparation method of Organic-inorganic composite water-miscible paint, comprises the following steps: by iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid and DMF carry out polyreaction under hydrothermal conditions, obtain metal-organic framework material; Nano titanium oxide dispersion and talcum powder is added in sodium silicate solution, first time adds described metal-organic framework material, silicon dioxide gel after stirring, dispersion agent, flow agent, defoamer, non-ionic emulsifier liquid, benzene emulsion, sodium acetate and water, second time stirs, and obtains Organic-inorganic composite water-miscible paint.
Preferably, described iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid, DMF, water glass, non-ionic emulsifier liquid, benzene emulsion, silicon dioxide gel, nano titanium oxide dispersion, sodium acetate, defoamer, flow agent, dispersion agent and talcous weight ratio are 1 ~ 3: 2 ~ 6: 0.05 ~ 0.1: 0.05 ~ 0.1: 0.2 ~ 0.6: 30 ~ 40: 0.2 ~ 0.3: 2 ~ 8: 5 ~ 10: 3 ~ 8: 0.1 ~ 0.2: 0.15 ~ 0.3: 0.15 ~ 0.3: 1 ~ 1.5: 10 ~ 13.
Preferably, described iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid, DMF, water glass, non-ionic emulsifier liquid, benzene emulsion, silicon dioxide gel, nano titanium oxide dispersion, sodium acetate, defoamer, flow agent, dispersion agent and talcous weight ratio are 2 ~ 3: 4 ~ 5: 0.05 ~ 0.1: 0.05 ~ 0.1: 0.3 ~ 0.5: 30 ~ 35: 0.25 ~ 0.3: 3 ~ 5: 6 ~ 8: 4 ~ 6: 0.15 ~ 0.2: 0.2 ~ 0.3: 0.15 ~ 0.2: 1 ~ 1.5: 11 ~ 13.
Preferably, obtain in the step of metal-organic framework material, the temperature of polyreaction is 140 ~ 160 DEG C, and the time of polyreaction is 8 ~ 20 hours.
Preferably, the stirring velocity that first time stirs is 2000 ~ 3000r/m, and churning time is 10 ~ 40 minutes.
Preferably, the stirring velocity that second time stirs is 800 ~ 900r/m, and churning time is 15 ~ 30 minutes.
Preferably, described dispersion agent is polyacrylamide.
Preferably, described flow agent is cellaburate.
The invention provides a kind of Organic-inorganic composite water-miscible paint and preparation method thereof, prepared by following raw material: water 25 ~ 45 weight part, iron powder 1 ~ 3 weight part, 1, 3, 5-benzenetricarboxylic acid 2 ~ 6 weight part, hydrofluoric acid 0.05 ~ 0.1 weight part, nitric acid 0.05 ~ 0.1 weight part, N, dinethylformamide 0.2 ~ 0.6 weight part, water glass 30 ~ 40 weight part, non-ionic emulsifier liquid 0.2 ~ 0.3 weight part, benzene emulsion 2 ~ 8 weight part, silicon dioxide gel 5 ~ 10 weight part, nano titanium oxide dispersion 3 ~ 8 weight part, sodium acetate 0.1 ~ 0.2 weight part, defoamer 0.15 ~ 0.3 weight part, flow agent 0.15 ~ 0.3 weight part, dispersion agent 1 ~ 1.5 weight part, talcum powder 10 ~ 13 weight part.Compared with prior art, the present invention does inorganic filming substance with water-soluble metasilicate, then composite with metal-organic framework material (MOF), obtains Organic-inorganic composite water-miscible paint.Because metal-organic framework material has Heat stability is good, pore passage structure in order, in hole, can many peculiar properties such as modified with functional group be carried out with surface, thus make water-miscible paint have satisfactory stability, resistance to elevated temperatures and sticking power.
Accompanying drawing explanation
Fig. 1 is the TG analysis chart of Organic-inorganic composite water-miscible paint prepared by the embodiment of the present invention 1.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of Organic-inorganic composite water-miscible paint, prepared by following raw material: water 25 ~ 45 weight part, iron powder 1 ~ 3 weight part, 1, 3, 5-benzenetricarboxylic acid 2 ~ 6 weight part, hydrofluoric acid 0.05 ~ 0.1 weight part, nitric acid 0.05 ~ 0.1 weight part, N, dinethylformamide 0.2 ~ 0.6 weight part, water glass 30 ~ 40 weight part, non-ionic emulsifier liquid 0.2 ~ 0.3 weight part, benzene emulsion 2 ~ 8 weight part, silicon dioxide gel 5 ~ 10 weight part, nano titanium oxide dispersion 3 ~ 8 weight part, sodium acetate 0.1 ~ 0.2 weight part, defoamer 0.15 ~ 0.3 weight part, flow agent 0.15 ~ 0.3 weight part, dispersion agent 1 ~ 1.5 weight part, talcum powder 10 ~ 13 weight part.
Preferably, described Organic-inorganic composite water-miscible paint is prepared by following raw material: water 30 ~ 40 weight part, iron powder 2 ~ 3 weight part, 1, 3, 5-benzenetricarboxylic acid 4 ~ 5 weight part, hydrofluoric acid 0.05 ~ 0.1 weight part, nitric acid 0.05 ~ 0.1 weight part, N, dinethylformamide 0.3 ~ 0.5 weight part, water glass 30 ~ 35 weight part, non-ionic emulsifier liquid 0.25 ~ 0.3 weight part, benzene emulsion 3 ~ 5 weight part, silicon dioxide gel 6 ~ 8 weight part, nano titanium oxide dispersion 4 ~ 6 weight part, sodium acetate 0.15 ~ 0.2 weight part, defoamer 0.2 ~ 0.3 weight part, flow agent 0.15 ~ 0.2 weight part, dispersion agent 1 ~ 1.5 weight part, talcum powder 11 ~ 13 weight part.
Accordingly, the present invention also provides a kind of preparation method of Organic-inorganic composite water-miscible paint, comprises the following steps: by iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid and DMF carry out polyreaction under hydrothermal conditions, obtain metal-organic framework material; Nano titanium oxide dispersion and talcum powder is added in sodium silicate solution, first time adds described metal-organic framework material, silicon dioxide gel after stirring, dispersion agent, flow agent, defoamer, non-ionic emulsifier liquid, benzene emulsion, sodium acetate and water, second time stirs, and obtains Organic-inorganic composite water-miscible paint.
Preferably, obtain in the step of metal-organic framework material, the temperature of polyreaction is preferably 140 ~ 160 DEG C, and the time of polyreaction is preferably 8 ~ 20 hours.The concentration of described hydrofluoric acid is preferably 35%, and the concentration of described nitric acid is preferably 65%.Preferably, the step obtaining metal-organic framework material is specially: by iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid, N, dinethylformamide and water add mixing and stirring in reactor, add a cover after moving to stainless steel cauldron sealing, place in electric drying oven with forced convection and react, obtain metal-organic framework material.
Metal-organic framework material (MOF) prepared by the present invention is the important component part of water-miscible paint solids component.Metal-organic framework materials (Metal-OrganicFrameworks, MOFs) is class I organic-inorganic hybridized material, is formed, generally have changeable topological framework and physicochemical property by organic ligand and inorganic metal cell formation.In the reaction, metal ion and organic ligand carry out framework coordination.The MOF of above-mentioned raw materials synthesis is MOF-5, with Fe ion for the coordination of atoms metal center, has the advantage of Heat stability is good.Fe powder is the central element of coordination, and 1,3,5-hydrofluoric acid and nitric acid dissolve Fe powder make it become ionic state, is that organic materials carries out coordination combination with 1,3,5-benzenetricarboxylic acid, DMF.The distribution of this metal-organic framework material has vital role for the homogeneity of Organic-inorganic composite water-miscible paint, and it can improve the impact strength of coating, and its supporting structure is present in inorganic coating and makes the resistance to elevated temperatures of coating better simultaneously.This material part intermolecular forces is extremely strong, and Stability Analysis of Structures, greatly strengthen the resistance to elevated temperatures of enamelled coating.Wherein, DMF can also increase stability and the polymerization degree of material, thus enhances the intensity of metal-organic framework material.
In the process preparing Organic-inorganic composite water-miscible paint, the present invention, using water-soluble metasilicate, silicon dioxide gel as inorganic phase, changes into the uniform film of inorganic phase at non-ionic emulsifier liquid and benzene emulsion effect lactogenesis.Because water glass and earth silicon material all have O-Si-O key, complex fire resistant water-miscible paint is made to have good sticking power.
Described nano titanium oxide (TiO
2) dispersion and talcum powder be resistant to elevated temperatures filler, TiO
2enhance intensity and the hardness of polymkeric substance; Talcum powder not only increases the hardness of complex fire resistant water-miscible paint, and effectively enhances sticking power.
Dispersion agent is a kind of interfacial agent simultaneously in molecule with lipophilicity and wetting ability two kinds of opposite nature, can homogeneous dispersion be difficult to be dissolved in the mineral dye of liquid and the solid particulate of pigment dyestuff, also can prevent sedimentation and the cohesion of solid particulate simultaneously, form stable material needed for suspension.Adding dispersion agent in coating can contracting floating, and prevent flocculation, prevent sedimentation, the present invention preferably uses polyacrylamide.Polyacrylamide makes organic metal framework material and inorganic water glass and earth silicon material form micro-emulsion polymerization, thus forms the fire resistant water-based paint of Organic-inorganic composite.
Described flow agent is the auxiliary agent in a kind of conventional coating industry, and coating can be impelled when emulsification film forming to form smooth, smooth, a uniform film.The present invention preferably uses cellaburate as flow agent.
Described defoamer has lower surface tension and higher surfactivity, can eliminate the foam material in water-miscible paint.Defoamer kind is a lot, and as organo-siloxane, imines and amides etc., have antifoaming speed fast and can adapt to the feature of high temperature, the present invention preferably uses organo-siloxane.
The non-ionic emulsifier liquid that the present invention adopts is preferably BASF polyoxyethylene nonylphenol ether 25, is preferably purchased from Shanghai Jinin trade Co., Ltd.
Described sodium acetate, as buffer solvent, can adjust metal-organic framework material and be coupled to potential of hydrogen in mineral silicate emulsion, ensure the smoothness of organic phase and inorganic phase emulsification.
In the preparation process of Organic-inorganic composite water-miscible paint, the water of employing is preferably deionized water.
In order to ensure that Organic-inorganic composite water-miscible paint has good performance, the weight ratio of the present invention to each raw material controls, described iron powder, 1, 3, 5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid, N, dinethylformamide, water glass, non-ionic emulsifier liquid, benzene emulsion, silicon dioxide gel, nano titanium oxide dispersion, sodium acetate, defoamer, flow agent, dispersion agent and talcous weight ratio are preferably 1 ~ 3: 2 ~ 6: 0.05 ~ 0.1: 0.05 ~ 0.1: 0.2 ~ 0.6: 30 ~ 40: 0.2 ~ 0.3: 2 ~ 8: 5 ~ 10: 3 ~ 8: 0.1 ~ 0.2: 0.15 ~ 0.3: 0.15 ~ 0.3: 1 ~ 1.5: 10 ~ 13.Preferred, described iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid, DMF, water glass, non-ionic emulsifier liquid, benzene emulsion, silicon dioxide gel, nano titanium oxide dispersion, sodium acetate, defoamer, flow agent, dispersion agent and talcous weight ratio are 2 ~ 3: 4 ~ 5: 0.05 ~ 0.1: 0.05 ~ 0.1: 0.3 ~ 0.5: 30 ~ 35: 0.25 ~ 0.3: 3 ~ 5: 6 ~ 8: 4 ~ 6: 0.15 ~ 0.2: 0.2 ~ 0.3: 0.15 ~ 0.2: 1 ~ 1.5: 11 ~ 13.
Preferably, the stirring velocity that first time stirs is preferably 2000 ~ 3000r/m, is more preferably 2200 ~ 2800r/m, is more preferably 2500r/m; The churning time that first time stirs is preferably 10 ~ 30 minutes, is more preferably 20 ~ 30 minutes.The stirring velocity that second time stirs is preferably 800 ~ 900r/m, and the churning time that second time stirs is preferably 15 ~ 30 minutes, is more preferably 20 ~ 30 minutes.
As can be seen from above scheme, the present invention does inorganic filming substance with water-soluble metasilicate, then composite with metal-organic framework material (MOF), obtains Organic-inorganic composite water-miscible paint.Due to metal-organic framework material there is Heat stability is good, pore passage structure is orderly, in hole and surface can carry out many peculiar properties such as modified with functional group, thus improve the stability of water-miscible paint, resistance to elevated temperatures and sticking power.Experimental result shows, Organic-inorganic composite water-miscible paint prepared by the present invention has good water tolerance, sticking power, snappiness, impact strength and resistance to elevated temperatures.
In order to understand the present invention further, be described in detail to technical scheme provided by the invention below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
The raw material that the embodiment of the present invention adopts and chemical reagent are commercial.
The non-ionic emulsifier liquid that the embodiment of the present invention adopts is BASF polyoxyethylene nonylphenol ether 25, is purchased from Shanghai Jinin trade Co., Ltd.
Embodiment 1
Prepare water-miscible paint in the steps below successively:
1, by weight containing following component: water 32% (first part's water: 12%, second section water 10%, Part III water 10%), iron powder 3%, 1,3,5-benzenetricarboxylic acid 5%, hydrofluoric acid (35%) 0.1%, nitric acid (65%) 0.1%, DMF 0.5%, water-soluble metasilicate 30%, silicon dioxide gel 6%, non-ionic emulsifier liquid 0.3%, benzene emulsion 3%, nano-TiO
2dispersion 5%, sodium acetate 0.15%, defoamer (organo-siloxane) 0.3%, flow agent (cellaburate) 0.15%, dispersion agent (polyacrylamide) 1.5%, talcum powder 12%.
2, by iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid (35%), nitric acid (65%), N, dinethylformamide and first part's water add mixing and stirring in reactor, add a cover after moving to stainless steel cauldron sealing, place electric drying oven with forced convection 150 DEG C reaction 12 hours.
3, water miscible sodium silicate solution and second section water are added low speed dispersion in emulsifying kettle, stir 10 minutes.Then add nano titanium oxide dispersion, talcum powder, under high shear force (2500r/m) effect, dispersion 30 minutes, makes fineness be less than 50um.
4, the product after (2) reactor is mixed in the emulsifying kettle in (3), add silicon dioxide gel again, dispersion agent (polyacrylamide), flow agent (cellaburate), defoamer (organo-siloxane), non-ionic emulsifier liquid, benzene emulsion 3%, sodium acetate and Part III water fully mix, middling speed (800 ~ 900r/m) stirs 20 minutes, is namely prepared into Organic-inorganic composite water-miscible paint.General placement 24h gets final product construction application.
Embodiment 2
Prepare water-miscible paint in the steps below successively:
1, mark contains following component by weight: water 35% (first part's water: 15%, second section water 10%, Part III water 10%), iron powder 2%, 1,3,5-benzenetricarboxylic acid 4%, hydrofluoric acid (35%) 0.1%, nitric acid (65%) 0.1%, DMF 0.5%, water-soluble metasilicate 35%, silicon dioxide gel 8%, non-ionic emulsifier liquid 0.3%, benzene emulsion 5%, nano-TiO
2dispersion 5%, sodium acetate 0.2%, defoamer (organo-siloxane) 0.3%, flow agent (cellaburate) 0.15%, dispersion agent (polyacrylamide) 1.5%, talcum powder 12%.
2, by iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid (35%), nitric acid (65%), N, dinethylformamide and first part's water add mixing and stirring in reactor, add a cover after moving to stainless steel cauldron sealing, place electric drying oven with forced convection 150 DEG C reaction 12 hours.
3, water miscible sodium silicate solution and second section water are added low speed dispersion in emulsifying kettle, stir 10 minutes.Then add nano titanium oxide dispersion, talcum powder, under high shear force (2500r/m) effect, dispersion 30 minutes, makes fineness be less than 50um.
4, the product after (2) reactor is mixed in the emulsifying kettle in (3), add silicon dioxide gel again, dispersion agent (polyacrylamide), flow agent (cellaburate), defoamer (organo-siloxane), non-ionic emulsifier liquid, benzene emulsion 3%, sodium acetate and Part III water fully mix, middling speed (800 ~ 900r/m) stirs 20 minutes, is namely prepared into Organic-inorganic composite water-miscible paint.General placement 24h gets final product construction application.
Embodiment 3
Prepare water-miscible paint in the steps below successively:
1, mark contains following component by weight: water 40% (first part's water: 20%, second section water 10%, Part III water 10%), iron powder 3%, 1,3,5-benzenetricarboxylic acid 4%, hydrofluoric acid (35%) 0.1%, nitric acid (65%) 0.1%, DMF 0.5%, water-soluble metasilicate 35%, silicon dioxide gel 8%, non-ionic emulsifier liquid 0.3%, benzene emulsion 5%, nano-TiO
2dispersion 5%, sodium acetate 0.2%, defoamer (organo-siloxane) 0.3%, flow agent (cellaburate) 0.15%, dispersion agent (polyacrylamide) 1.5%, talcum powder 12%.
2, by iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid (35%), nitric acid (65%), N, N
-dimethyl formamide and first part's water add mixing and stirring in reactor, add a cover after moving to stainless steel cauldron sealing, place electric drying oven with forced convection 150 DEG C reaction 12 hours.
3, water miscible sodium silicate solution and second section water are added low speed dispersion in emulsifying kettle, stir 10 minutes.Then add nano titanium oxide dispersion, talcum powder, under high shear force (2500r/m) effect, dispersion 30 minutes, makes fineness be less than 50um.
4, the product after (2) reactor is mixed in the emulsifying kettle in (3), add silicon dioxide gel again, dispersion agent (polyacrylamide), flow agent (cellaburate), defoamer (organo-siloxane), non-ionic emulsifier liquid, benzene emulsion 3%, sodium acetate and Part III water fully mix, middling speed (800 ~ 900r/m) stirs 20 minutes, is namely prepared into Organic-inorganic composite water-miscible paint.General placement 24h gets final product construction application.
Respectively following performance test is carried out to Organic-inorganic composite water-miscible paint prepared by embodiment 1 ~ 3:
1, the test of coating adhesion
Carry out polishing on the tinplate surface being of a size of 120mm × 50mm × 0.3mm, after clean and drying treatment, Organic-inorganic composite water-miscible paint embodiment prepared equably with painting brush is coated in test plate (panel) surface, Air drying is after 7 days, lattice are drawn with drawing lattice device, then be adjacent to scotch tape and draw lattice place, pull off adhesive tape again, observe the situation that paint film destroys, judge the rank of its sticking power.
2, water-resistant coating test
By GB/T 1733-1993 standard testing.
Carry out polishing at the surface of steel plate being of a size of 120mm × 50mm × 0.8mm, after clean and drying treatment, test plate (panel) surface is coated in the Organic-inorganic composite water-miscible paint that embodiment is prepared by the wet film preparing device that specification is 100 μm, Air drying is after 7 days, test plate (panel) applies paraffin and the rosin blend edge sealing of 1: 1 before throwing examination, edge sealing width 2 ~ 3mm.Add distilled water in a reservoir, be immersed in the water 2/3rds of model.Observe the situation of test plate (panel), record time when changing.
3, thermogravimetric (TG) is analyzed
Test with the TG 209F type thermogravimetric analyzer that NETZSCH company produces, test condition is: sample quality 5 ~ 10mg, and under air atmosphere, temperature rise rate is 20 DEG C/min, and temperature range is 30 DEG C ~ 900 DEG C.As shown in Figure 1, found by Fig. 1, when temperature is when close to 900 DEG C, the remaining quality of coating is more than 93%, and thermosteresis is less for the TG analysis chart of Organic-inorganic composite water-miscible paint prepared by embodiment 1.
The over-all properties of Organic-inorganic composite water-miscible paint prepared by embodiment 1 prepared by the embodiment of the present invention 1 ~ 3 is as shown in table 1.
The over-all properties of Organic-inorganic composite water-miscible paint prepared by table 1 embodiment 1 ~ 3
As can be seen from Table 1, the Organic-inorganic composite water-miscible paint that prepared by the embodiment of the present invention has good water tolerance, sticking power, snappiness, impact strength and resistance to elevated temperatures.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. an Organic-inorganic composite water-miscible paint, is characterized in that, is prepared by following raw material:
Water 25 ~ 45 weight part, iron powder 1 ~ 3 weight part, 1, 3, 5-benzenetricarboxylic acid 2 ~ 6 weight part, hydrofluoric acid 0.05 ~ 0.1 weight part, nitric acid 0.05 ~ 0.1 weight part, N, dinethylformamide 0.2 ~ 0.6 weight part, water glass 30 ~ 40 weight part, non-ionic emulsifier liquid 0.2 ~ 0.3 weight part, benzene emulsion 2 ~ 8 weight part, silicon dioxide gel 5 ~ 10 weight part, nano titanium oxide dispersion 3 ~ 8 weight part, sodium acetate 0.1 ~ 0.2 weight part, defoamer 0.15 ~ 0.3 weight part, flow agent 0.15 ~ 0.3 weight part, dispersion agent 1 ~ 1.5 weight part, talcum powder 10 ~ 13 weight part.
2. Organic-inorganic composite water-miscible paint according to claim 1, is characterized in that, is prepared by following raw material:
Water 30 ~ 40 weight part, iron powder 2 ~ 3 weight part, 1, 3, 5-benzenetricarboxylic acid 4 ~ 5 weight part, hydrofluoric acid 0.05 ~ 0.1 weight part, nitric acid 0.05 ~ 0.1 weight part, N, dinethylformamide 0.3 ~ 0.5 weight part, water glass 30 ~ 35 weight part, non-ionic emulsifier liquid 0.25 ~ 0.3 weight part, benzene emulsion 3 ~ 5 weight part, silicon dioxide gel 6 ~ 8 weight part, nano titanium oxide dispersion 4 ~ 6 weight part, sodium acetate 0.15 ~ 0.2 weight part, defoamer 0.2 ~ 0.3 weight part, flow agent 0.15 ~ 0.2 weight part, dispersion agent 1 ~ 1.5 weight part, talcum powder 11 ~ 13 weight part.
3. a preparation method for Organic-inorganic composite water-miscible paint, is characterized in that, comprises the following steps:
Iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid and DMF are carried out polyreaction under hydrothermal conditions, obtains metal-organic framework material;
Nano titanium oxide dispersion and talcum powder is added in sodium silicate solution, first time adds described metal-organic framework material, silicon dioxide gel after stirring, dispersion agent, flow agent, defoamer, non-ionic emulsifier liquid, benzene emulsion, sodium acetate and water, second time stirs, and obtains Organic-inorganic composite water-miscible paint.
4. preparation method according to claim 3, it is characterized in that, described iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid, DMF, water glass, non-ionic emulsifier liquid, benzene emulsion, silicon dioxide gel, nano titanium oxide dispersion, sodium acetate, defoamer, flow agent, dispersion agent and talcous weight ratio are 1 ~ 3: 2 ~ 6: 0.05 ~ 0.1: 0.05 ~ 0.1: 0.2 ~ 0.6: 30 ~ 40: 0.2 ~ 0.3: 2 ~ 8: 5 ~ 10: 3 ~ 8: 0.1 ~ 0.2: 0.15 ~ 0.3: 0 ~ 0.3: 1 ~ 1.5: 10 ~ 13.
5. preparation method according to claim 3, it is characterized in that, described iron powder, 1,3,5-benzenetricarboxylic acid, hydrofluoric acid, nitric acid, DMF, water glass, non-ionic emulsifier liquid, benzene emulsion, silicon dioxide gel, nano titanium oxide dispersion, sodium acetate, defoamer, flow agent, dispersion agent and talcous weight ratio are 2 ~ 3: 4 ~ 5: 0.05 ~ 0.1: 0.05 ~ 0.1: 0.3 ~ 0.5: 30 ~ 35: 0.25 ~ 0.3: 3 ~ 5: 6 ~ 8: 4 ~ 6: 0.15 ~ 0.2: 0.2 ~ 0.3: 0.15 ~ 0.2: 1 ~ 1.5: 11 ~ 13.
6. preparation method according to claim 3, is characterized in that, obtains in the step of metal-organic framework material, and the temperature of polyreaction is 140 ~ 160 DEG C, and the time of polyreaction is 8 ~ 20 hours.
7. preparation method according to claim 3, is characterized in that, the stirring velocity that first time stirs is 2000 ~ 3000r/m, and churning time is 10 ~ 40 minutes.
8. preparation method according to claim 3, is characterized in that, the stirring velocity that second time stirs is 800 ~ 900r/m, and churning time is 15 ~ 30 minutes.
9. preparation method according to claim 3, is characterized in that, described dispersion agent is polyacrylamide.
10. preparation method according to claim 3, is characterized in that, described flow agent is cellaburate.
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